CN103845924A - Parallel flow falling film extraction process and equipment - Google Patents

Parallel flow falling film extraction process and equipment Download PDF

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Publication number
CN103845924A
CN103845924A CN201210519191.3A CN201210519191A CN103845924A CN 103845924 A CN103845924 A CN 103845924A CN 201210519191 A CN201210519191 A CN 201210519191A CN 103845924 A CN103845924 A CN 103845924A
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extraction
equipment
liquid
filler
liquid film
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CN103845924B (en
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翁慧超
杨家麒
尹应武
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TH-UNIS Insight Co., Ltd.
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Xiamen University
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Abstract

The invention relates to a novel parallel flow extraction process and efficient extraction equipment. The equipment comprises a heavy-phase charging hole (1), a light-phase charging hole (2), a liquid distributor (3), packing (4), equipment (5) filled with the packing, a mixed liquid discharging hole (6), a clarifying tank (7), a light-phase discharging hole (8) and a heavy-phase outlet (9). The extraction speed can be remarkably improved by the aid of a spherical or tubular packing tower. Two solutions flow from the tower top or are mixed, and then enter a packing layer through the liquid distributor; under the action of self power and great liquid-gas specific gravity difference, the mixed liquid is scattered on the surface of the packing of a spherical metal screen to form a film, so that great two-phase contact area is formed. In an ideal low-energy-consumption and high-efficiency effective liquid-liquid contact mode, the technical equipment can be used for systems for extraction or reaction extraction and the like.

Description

One also flows falling liquid film extraction process and equipment
Technical field
The present invention relates to mass transfer and separation engineering technical field.
Background technology
Extraction has been widely used in the fields such as petrochemical industry, pharmacy, metallurgy and environment as the main separate mode of chemical industry.Current general extraction equipment has: 1) mixer-settler takes up room greatly, and operating cost is high; 2) packed tower applicable surface is narrow, and extraction efficiency is low; 3) oscillating screen plate tower difficulty of processing is large, and treating capacity is little; 4) centrifugal extractor is applicable to the little system of difference in specific gravity, and treating capacity is little, and energy consumption is large.For a long time, abstraction technique and be equipped in improve extraction rate, reduction equipment size, reduce height and number of unit, reduction energy consumption aspect, always without breakthrough.
Summary of the invention
The present invention is based on following analysis, hope can be invented the technology and device effectively addressing the above problem:
In common liquid-liquid extraction system, decentralized photo and continuous phase are all liquid phases, and drop is coalescence very easily, cause the problems such as two-phase contact area is little, extraction rate is low.Although the equipment of the extra input such as oscillating screen plate tower, stirring extractor, centrifugal extractor energy has to a certain degree improved extraction rate, extraction rate is still difficult satisfactory, and has brought the problems such as energy consumption is high, noise is large.
We had once invented a kind of spherical metal wire packing (patent No.: 200610086495.X). find that it has handling ease, materials are saved, the large resistance of flux is little, the plurality of advantages such as separating effect height, eyelet and sphere diameter can be adjusted according to the requirement of system, are particularly suitable for rectification system.We find to select Ball-type packing as extraction stuffing, at extract and extractant and flow falling liquid film extraction or counter-current extraction in the situation that, can greatly improve extraction efficiency, obtain the good effect of accident that is different from common extraction pattern and common filler extraction effect completely.Found spherical wire packing and and to flow falling liquid film extraction be potential and the most energy-efficient a kind of equipment for extraction and technology, may extensively substitute existing extraction equipment.Based on the above results, we propose one and flow falling liquid film extraction mode, and adopt spherical metal wire packing, have invented a kind of novel extraction technique and equipment with high extraction rate.
And flow falling liquid film extraction and be different from traditional liquid-liquid counter-current extraction, two kinds of liquid separately or mix the liquid distribution trough by tower top and wander down, due to be first continuous air mutually in spray disperse two kinds of liquid phases simultaneously, by self gravity and dynamic action and the huge liquid-gas ratio method of double differences, liquid material very easily disperses in gas phase, two kinds of drops or the liquid film fallen on Ball-type packing can be constantly descending along Ball-type packing under self gravitation and capillary continuous action, disperse, distribute, film forming, fully contact, on two kinds, surface of spherical silk screen, liquid film constantly alternately forms and upgrades, under gravity and capillary effect, liquid film thickens gradually, final formation drop or liquid drip are fallen next silk screen spherome surface, form new liquid film, continuous film forming through some balls can reach balance very soon, produce desirable low energy consumption and high efficiency effect of extracting, by up and down or left and right plural serial stage, be easy to meet extraction requirement.
Brief description of the drawings
Fig. 1 Ball-type packing structural representation
The tubular filling-material structure schematic diagram of Fig. 2
Fig. 3 also flows falling liquid film equipment for extraction schematic diagram
Heavy phase charging aperture (1), light phase charging aperture (2), liquid distribution trough (3), filler (4), the equipment (5) of filling filler, mixed liquor discharging opening (6), defecator (7), light phase discharging opening (8), heavy out (9).
Fig. 4 equipment for extraction multi-stage countercurrent series connection schematic diagram
Light phase materials import (1), heavy phase material inlet (2), liquid distribution trough (3), filler (4), the equipment (5) of filling filler, mixed liquor discharging opening (6), defecator (7), liquor pump (8), light phase one-level equilibrium liquid discharging (9), light phase one-level equilibrium liquid charging (10), light phase secondary equilibrium liquid discharging (11), light phase secondary equilibrium liquid charging (12), heavy phase discharging opening (13), light phase discharging opening (14).
Fig. 5 equipment for extraction multistage cross flow series connection schematic diagram
Liquid charging aperture to be extracted (1), solvent feed mouth (2-4), liquid distribution trough (5), filler (6), the equipment (7) of filling filler, liquid outlet to be extracted (8-10), defecator (11), solvent outlet (12-14).
Fig. 6 light with heavy phase liquid at filling surface distribution schematic diagram
Heavy phase liquid (1), spherical/tubular filler (2), light phase liquid (3).
Detailed description of the invention
Test 1 effect of extracting and evaluate control experiment 1
In 2000ml water, add elemental iodine 0.400g, and add KI 1.000g, be configured to the IKI aqueous solution of 200mg/L.Get wherein 160ml, be placed in 500ml beaker, use magnetic stirrer, rotor speed is 400r/min, the raffinate amount of iodine in 1.5 minutes sample analysis iodine water, and the data obtained is in table 1.
Test 2 effect of extracting and evaluate control experiment 2
The IKI aqueous solution 2000ml of same concentration in preparation experiment 1, is all placed in the plastic beaker of 5000ml, adds 1000ml cyclohexane.Use the shaft that axial length is 5.6cm to stir, rotating speed is 400r/min, the raffinate amount of iodine in 1.5 minutes sample analysis iodine water, and the data obtained is referring to table 1.
Test 3 spherical wire packings and flow falling liquid film experiment
Same IKI aqueous solution 2000ml in preparation experiment 1, prepare 1000ml cyclohexane simultaneously, in the tower that Φ 25 Ball-type packings are housed, carry out and flow falling liquid film extraction experiments, tower diameter 105mm, packed height is 95cm, iodine discharge 200L/h, cyclohexane flow 100L/h, at the bottom of tower, discharging is returned tower top with pump.The raffinate amount of iodine in 1.5 minutes sample analysis iodine water, the data obtained is referring to table 1.
Test 4 Intalox metal tower packing cocurrent extraction experiments
To test replacement in 3 is #25 rectangular saddle ring, repeats to test the experimental procedure in 3, and the data obtained is referring to table 1.
Test 5 spherical wire packings and flow falling liquid film extraction experiments
In 5000ml water, add elemental iodine 0.200g, and add KI 0.500g, be configured to the IKI aqueous solution of 40mg/L.In gained solution and the tower of 500ml cyclohexane in embodiment 3, dosage repeats and flows falling liquid film experiment, analyzes the raffinate amount of iodine at the bottom of tower, and the data obtained is referring to table 2.
Test 6 spherical wire packing adverse current falling liquid film extraction experiments
The same IKI aqueous solution in preparation experiment 5, does counter-current extraction experiment in the tower in experiment 3, analyze the raffinate amount of iodine, and the data obtained is referring to table 2.
Test 7 Intalox metal tower packing cocurrent extraction experiments
The same IKI aqueous solution in preparation experiment 5, does in the tower in experiment 4 and flows falling liquid film experiment, analyzes the raffinate amount of iodine at the bottom of tower, and the data obtained is referring to table 2.
Test the tubular filler cocurrent extraction experiment of 814 order
To test replacement in 3 is the tubular filler of 14 order φ 30mm, and the same IKI aqueous solution in configuration experiment 5, repeats to test the experimental procedure in 3, and the data obtained is referring to table 2.
Test the tubular filler cocurrent extraction experiment of 98 order
To test replacement in 3 is the tubular filler of 8 order φ 30mm, and the same IKI aqueous solution in configuration experiment 5, repeats to test the experimental procedure in 3, and the data obtained is referring to table 2.
Test 10 Intalox metal tower packing counter-current extraction experiments
The same IKI aqueous solution in preparation experiment 5, does counter-current extraction experiment in the tower in embodiment 4, analyze the raffinate amount of iodine at the bottom of tower., the iodine water in tower and cyclohexane are taken out meanwhile, again at the bottom of tower top and tower, pass into respectively, carry out secondary, three times, four times, five times counter-current extractions, acquired results is referring to table 3.
Table 1 is tested 1-4 analysis result
Figure BSA00000818309000041
Table 2 is tested 5-9 analysis result (content of iodine in liquid to be extracted: 40mg/L)
Figure BSA00000818309000051
Table 3 is tested 10 analysis results (content of iodine in liquid to be extracted: 40mg/L)
(rectangular saddle ring counter-current extraction)
Figure BSA00000818309000052

Claims (9)

1. a falling liquid film equipment for extraction, it comprises the heavy phase charging aperture (1) on top, light phase charging aperture (2), liquid distribution trough (3), filler (4), the equipment (5) of filling filler, mixed liquor discharging opening (6), defecator (7), heavy phase discharging opening (8), light phase export (9).
2. falling liquid film equipment for extraction according to claim 1, is characterized in that: filler used can be any single filler or load in mixture filler.
3. according to claim 1 and flow falling liquid film extraction or counter-current extraction and equip preferably spherical and tubular metal wire packing or load in mixture filler of in-built filler, the barrel hole size of silk screen between 0.1mm between 6mm.
4. falling liquid film equipment for extraction according to claim 1, it is characterized in that: heavy phase material and light phase materials equipment can be simultaneously from top and flow access arrangement, can be first after the preliminary mixing in liquid distribution trough (3) upper end, flow down by liquid distribution trough again, also can directly spray and be distributed to filling surface, extraction stuffing can partially or completely be exposed to air mutually in, can be used as preferred extraction pattern.
5. spherical or tubular wire packing equipment for extraction according to claim 1, is characterized in that as required: heavy phase material can be from its top feed, and light phase materials is sent into from bottom, carries out counter-current extraction, and filler is immersed in liquid phase.
6. falling liquid film equipment for extraction according to claim 1, is characterized in that: the container of filling filler can be that tower also can be used still and other any containers, can also be the crosscurrent extraction tower of transformation.
7. falling liquid film equipment for extraction according to claim 1, according to the needs of extraction progression, can multiple falling liquid film equipment for extraction up and down or left and right series connection, form multi-stage counter current extraction, multistage cocurrent extraction or multistage cross flow extraction, be not subject to device shaped and big or small restriction.
8. falling liquid film equipment for extraction according to claim 1, liquid distribution trough (3) can be the common liquid distribution apparatus such as disc type liquid distribution trough, tank type liquid distributor, tubular liquid distributor.
9. falling liquid film equipment for extraction according to claim 1, the height of defecator (7) is depending on the two phase stratification time, general not higher than 1/2 of packed height.
CN201210519191.3A 2012-12-07 2012-12-07 Parallel flow falling film extraction process and equipment Active CN103845924B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107803050A (en) * 2017-12-08 2018-03-16 中国科学院过程工程研究所 A kind of dynamic magnetic particle combination membrane extraction device and extracting process
CN109701297A (en) * 2019-03-05 2019-05-03 北京化工大学 A kind of hypergravity extraction and separation coupling device and application
CN115089998A (en) * 2022-06-01 2022-09-23 呈和科技股份有限公司 Organic matter static extraction device

Citations (4)

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Publication number Priority date Publication date Assignee Title
JPS63107704A (en) * 1986-10-24 1988-05-12 Kawasaki Steel Corp Extraction material and extraction method
CN101091902A (en) * 2006-06-23 2007-12-26 北京清华紫光英力化工技术有限责任公司 Dispersed piled spherical stuffing
CN201643778U (en) * 2010-02-11 2010-11-24 山西翔宇化工有限公司 Non-stirring type extracting tower
CN202289553U (en) * 2011-10-31 2012-07-04 宁波环洋化工有限公司 Device for recovering useable organic matter from waste oil generated by refined epoxy chloropropane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63107704A (en) * 1986-10-24 1988-05-12 Kawasaki Steel Corp Extraction material and extraction method
CN101091902A (en) * 2006-06-23 2007-12-26 北京清华紫光英力化工技术有限责任公司 Dispersed piled spherical stuffing
CN201643778U (en) * 2010-02-11 2010-11-24 山西翔宇化工有限公司 Non-stirring type extracting tower
CN202289553U (en) * 2011-10-31 2012-07-04 宁波环洋化工有限公司 Device for recovering useable organic matter from waste oil generated by refined epoxy chloropropane

Non-Patent Citations (1)

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Title
黄亚东: "《生物工程设备及操作技术》", 31 August 2008 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107803050A (en) * 2017-12-08 2018-03-16 中国科学院过程工程研究所 A kind of dynamic magnetic particle combination membrane extraction device and extracting process
CN107803050B (en) * 2017-12-08 2019-11-08 中国科学院过程工程研究所 A kind of dynamic magnetic particle combined films extraction equipment and extracting process
CN109701297A (en) * 2019-03-05 2019-05-03 北京化工大学 A kind of hypergravity extraction and separation coupling device and application
CN115089998A (en) * 2022-06-01 2022-09-23 呈和科技股份有限公司 Organic matter static extraction device
CN115089998B (en) * 2022-06-01 2023-12-26 呈和科技股份有限公司 Static extraction device for organic matters

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